Method of manufacturing distilled alcoholic liquors



tiitltdyldt' auf@ hid till 1 v tliimdiiit lididltlhd aiu h. por, s dnrcelea, il., assior to dtrial laboratories,l liitd. Whicago, iiil. a corporation of ola plieation dpril tu, lait, denial lilo.. tutti il im This invention relates to a ethod oi manufacturing distilled alcoholic liauors d, pieularly, to a method of materially accelerat the maturing thereof.y y

it has been believed for some time that the aging of alcoholic liquors is connected with the oxidation of certain constituents thereof and various'means have been proposed for accelerating this oxidation. it has now been discofvered that the aging of high alcoholic liquors, such as whiskey, brandy, and the lille, consists of two tes of oxidation. The hrst t has heretofore been carefully studied chemically, particularly in the worlr of the laboratory of the ureau of internal Revenue, which work was embodied in a report entitled The study oi' the changes nu to in whiskeys stored in woo by C. h. Crompton and L. M. Tolman, published in voie th-il. Journal of the american Checal Society, ldlld. The changes embodied in this type of oxidation are primarily the oxidation of alcohols st to aldehydes and then to acids, and the subsequent interaction of acids with alcohol to form esters. itt the same time, Acertain other aterials are extracted from the oalr contners to n. usual whisirey color.

The second type of oxidation or enge has now been discovered to occur in what are here entitled the congeneric substances oi the liuuor. These substances are the minute, highly arctic and haver-producing materials, hitherto unisolated, which produce the distinctive bouquet of the van rious whiskeys and other high alcoholic liquors. it is the changes in these materials which produce the matured or softened bouquet of the aged liquor. It has been discovered that the changes in these materials do not readily taire place in the presence of an excess of the remaining constituents of the whiskey, and apparently the changes are particularly inhibited by the presence ot alcohol. if, however, these congeneric materials be separated, or substantially concentrated, oxidation occurs much more readily. l

in accordance with this inventionn the congeners are separated from the bodyoi the whisirey, or a concentrate thereof is prepared, and this concentrate then contacted with air in small amounts to carry out the aging process, and the congeners are then returned to the main both? of liquor. This treatment materially increases the iodine number and acid value of the congeners and markedly affects the bouquet-producing dualities thereof. The amount of congeners obtain@ able is so small. that detailed chemical analysis thereof has been. impossible. i-ioWeyers there through te i stances are oily tters of acid reaction. When cold, the extracted congeners are greasy crystalline white materials. When heated to the melting point, they have a. light brown or yellow color. The greasy material has an iodine value of about a 37.7 and an acid value of about 3i. lifter treatment as hereinafter described, the iodine number increases to about 36 and the acid value to about at.

.ii diagraatic elevation/.with parts in seclo tion, of an apparatus for carrying out the invention is illustrated inthe drawing, in whichl and le represent d for holding the liquor, which may be of any suitable nber or capacity, such as 25th gallons, means for passing liquor iii from :w i im to di, means for passing air u i ai and means for condensing so far as possible volatiles contained in the air which has passed through the aerated liuuor fraction.

i; constructed of any suitable ate=lrial not adected by spirits, are substantially identical, but the interior construction is shown only roi' cui i., 'the drum is provided with a plurty cfscreens or perforated plates l, .the perali iterations of which may be any suitable diameter.; for instance, one-quarter inch. Upon the plates are piled any suitable materials which have the property of extracting concentrates of congeneric materials from the liquor. It is preferred to use 3@ curled beechwood shavings which have been thoroughly treated to remove all coloring and davoring matter therefrom. 'These shavings are readily obtained in coerciai quantities. en the hill drum has been filled as full as conveniently prac- '35l tic-able, the shavings will occupy about one-ftha of the vole oi' the u i i n en liquor has been introduced, the shavings will piclr up about onedfth additional vole and will hold about that proportion oi' liquid. The beechwood shavings ill appear particularly adapted to separating a concentrate rich in oils, and also are neutral or inert. @ther litre absorptive materials may be employed.

The drums are provided with means for passi5 ing oxygen, or air, through the shavings. This may be done by providing an air spreader which is connected with a source of air which is illustrated diagrannnaticaily by the line Li. the air preferably heated by passing through an airheating unit iii. lt is not necessary or preferred to use a great amount of air, but on the contrary, only gentle bio-adrig is desired. it the topiof "i draw-oh" line for the air is provide" to .a water-cooled GEES' denser 6 connected to a'liquid receiver 1. The liquid receiver is connected to both drums by the lines 8 and 88L controlled by valves 9 and 98L so that the condensate may be introduced into either drum as it is formed. If desired, however, the condensate may be retained and introduced into the final treated liquor before packaging.

Means are also provided for passing liquor from one drum to another. In the drawing, this is illustrated by the lines I4 and I4 connected to the pump l l. The line IB, metered with meter I5, passes the treated product to the cistern or barreling room when aeration is complete.

In carrying out the operation of the process, raw high-wines are pumped from the reservoir it through line I into one of the drums, say drum l, which has been previously lled with shavings, as indicated. The material is allowed to ,stand in the drum for a period of about one-half hour, or until the shavings are substantially saturated with congeneric materials. The bulk of the highwines is then pumped into the alternate drum ie, leaving upon the shavings an adsorbed concentrate of congeneric substances in the drum i. The term concentrate as here used simply .means that the congeneric substances are more concentrated on the shavings than they were in the main body of the liquor. The actual concentration of these substances is extremely small.l

Air is then passed through the drum in a gentle stream for a short period, say about 1/2 to' 2 hours,

' preferably about one hour. It is preferred to introduce air at a temperature sufficient that the saturated shavings are maintained at about 8090 F. Normally, this may be accomplished by heating the air to about 100 F. The air passing from the drum goes through the condenser ii and is discharged to the outside air and any condensate is collected in the receiver 1.

The term high-wines is used in the whiskey' trade to indicate the raw liquor. i

The amount of air used is quite small, although the amount thereof may vary widely. It is preferred to keep the amount as small as possible, in order that the amount of congeneric materials carried away in vapor form be reduced to a minimum. After the blowing is complete, the shavings are still wet and no material evaporation has taken place from them.

After this blowing period, the main body of the' iiquor is pumped from the drum l back into the drum l and the concentrate left in the drum Ia is then blown vin the same manner. This process is repeated as often as desired, normally 3 to 5' times. It has been discovered that the maximum efiiciency is obtained by blowing for about fiveto eight hours, although longer periods of blowing may be used, if desired. A preferred range is' from 6 to 8 hours. 0f course, when the main body of liquid is returned to a drum containing a concentrate already aerated, it should be held there long enough for interchange to take place between the essential oils in the shavings withV also high in aldehydes, including furfural. The

acids, however, are low and the esters are about the same as the original material. It is important to return this condensate to the main body of the liquor, inasmuch as it contains a considerable proportion of the essential flavoring and aromatic constituents.

The liquor may then be drawn o from the drums and stored in charred oak barrels of the' usual type. These directions are, of course, for American whiskey, and if Scotch whiskey is desired, 'the barrels need not be charred. After ninety days, whiskey of characteristics and bouquet substantially equal to that of four-year-old whiskey is produced and the acceleration is of about this order all along the line.

The process'may be used upon all high alcohol content (distilled) liquors of the whiskey and other types, including but not being limited to Bourbon, rye or Scotch whiskeys, rum, brandy and the '-like.4 and is unaffected by Whether the Ina-shis'sweet or sour. Other methods of separating the congenericmaterals from the main body of liquor may be used. rihe process is particularly adapted to be applied as a step in the movement of the liquor from the doubler to the cistern or barreling room. The step is in no sense rectification since nothing is added to or withdrawn from the liquor, nor is there any mixing of runs, so that no rectification tax is cpplicable.

As already set forth, the theory upon which the process operates is not thoroughly understood, `but'it is believed that the congeners which are concentrated in the material left upon the shavingsare oxidized in that environment. The effect is entirely different from that accomplished in the ordinary scr-called aging processes in which air or oxygen is pumped through an unfractionated body of liquor. i

The separation appears. to be a matter of surface tension, the oils being adsorbed upon the large surface of. the shavings. /They thus present an extremely large surface to the air current and readily undergo oxidation.

The foregoing detailed description has been given-for'clearness'of understanding only, and no unnecessary limitations should be understood therefrom, but the' appended claims should be construed asvzbroadly as permissible, in view of the prior art. Y

Y -This'case-'is a continuation in part of my copending application 723,267.

What IA claim as new, and desire to secure by Letters. Patent, is:

1. In thev manufacture of distilled alcoholic liquors, the steps of repeatedly contacting raw liquor with curled beechwood shavings for a period of the order of 4one-half hour, then withdrawing the body of the liquor, contacting the material absorbed upon the shavings with oxygen for a period of the order of one-half hour to oxidize the same without producing substantial evaporation therefrom, returning the main body of liquor` to the shavings after the blowing, and aging the 'so-treated liquor in oak containers.

2. The-method as set forth in claim 1, in which the concentration and blowing are repeated from three to' iive times.

-3.v The method as set forth in claim 1, in which the oxygen, vafter contacting the shavings is cooled to produce a condensate of volatile materials from-the alcoholic liquor, and the condensate is permanently Vreturned to the liquor.

zoA

4. Indalia manufacture of a. distilled alcoholic liquor, the steps ci concentrating congeneric substances oi the liquor upon a solid absorptive terial, removing the in body oi the liquor from the concentrate, oxidizing congeneric subing strearn including gaseous oxygen for a period oi" at least one-half hour, the period being wir. ciently long thoroughly to oxidize the congeneric substances, and sumciently short to avoid eyaporating the concentrate to approach ess, the amount oi evaporation being limited to the order of one ounce per gallon oi treated liquor during the entire blowing operation, and returning the oxidized concentrate to the main body of liquor.

5. The method as set forth in claim al, in which the oxygen which has contacted the concentrate is cooled to produce a condensate of material removed from the alcoholic liquor, and the condensate is permanently returned to the main body of liquor.

d. The method as set forth the liquor is whislrey.

71. ln the manufacture of a distilled alcoholic liquor, the stem oi contacting the liquor lor a period as lo as one-t to two hours with in claim i, in which curled beech-wood shavings, removing the main body oi liquor, except lor absorbed material upon the shavings, contacting the absorbed material with oxygen, to oxidize congeneric substances, ior stances in the concentrate by contact with a mova prolonged period without substantial. evaporation therefrom, and returning the main body of the liquor to the so-treated shavings.

8. The method as set forth in claim 'l'. in which the shavings are gently blown with air for a period ci` one-half to two hours, and in' which the separation of liquor from the shavings and blowing with air are repeated.

9. ln the manufacture of a distilled alcoholic liquor, the steps or concentrating congeneric substances oi the liquor on a solid absorptive material, removing the main body of the liquor from the concentrate, oxidizing congeneric substances in the concentrate by contact with a moving stream including gaseous oxygen lor a period oi at least one hour and not substantially longer than eight hours, whereby the congeneric substances are thoroughly oxidized, and returning the oxidized concentrate to the main body of liquor.

EDWIN E. COX. 

